Process for steam treating magnesium cement fibrous panels



July 12, 1960 w. L. PRIOR ETAL PROCESS FOR STEAM TREATING MAGNESIUM CEMENT FIBROUS PANELS Aii ,Sims e" PROCESS FOR STEAM TREATING Y e cEMEN'rFmRoUs rANELs William Lg.V Prior and HowardfJfSnelson, Newark, Ohio,

assgnors tofTectum Corporation,- Columbus, Ohio, a corporation of Ohio V` v- Y This invention relates Itothe formationv of structural *building material in the form of fibrous board composed of-,wood 4woolpor excelsior and v,a magnesium `cement binder; Morel particularly, the instant invention relates toprocedures whereby the setting time of the magnesium cement c an'be greatly' reduced and, at the same time, certain physical characteristics ofY theoproduct improved overs'imilar products made by presently known methods. 'I'he i nstant invention isv` particularly adapted for use in.A a continuous process wherein `the raw.Y materials are assembled, compounded, compressed and the. `cementitious'binderset or curedin a continuous operation; Y The continuous processing of'. such materialV has hitherto pre- As'entet:numerous problems, particularly iinsofar as the formulation and handling of the magnesium cement is GNESIUM concerned; fand whilemagnesiumcement panels arelcui'f Y rentlybeing manufacturedfin thiscountry in accordance with the rehings encourus raient No. 2,655,458,1the procedures involved@ require careful control.' overthe chemicalY activity of the .magnesiumgoxide and` apress Ior setting time froma maximurnof about lOl/z minutes 'to a"minimum-offabout 4'mi'nutes. As opposed to this, iniaccordance with the instant invention the press or setting time is reduced to a. maximums of about 5 minutes landeminimum of about 30 seconds withoptimum resu-lts' in' therangelof 60 -9O secoi'id's.'v `ln,additio`n,. the

chemical activityvfof'the magnesium :oxide becomesnm- :important and ,larry active oxide`may `be employed.

The magnesium @cen-lents to which this invention relates .are generally'kno-Wn asffmagnesiumoxysulfatelcemen and fma'gnesium oxychloridecement.z The former fis preferred and is `of the system MgO-,rMgSOii-IHZO, although -it will be understood that magnesiurnoxychloride cement may be readily substituted without departing from the spirit of our invention. VActually, thedesignation magnesiumoxysulfate cernen appears 4 to be a n misnomerin that the system is correctly identified as sul- 'phated ymagnesium hydroxide, made Abythe reactionfof magnesium oxide with a solution of magn`esium sulfate ,(Epsom salts). However, since fthe `designation mag- `nesium oxychloride is in general u'sagebothy in ltheitexts Aand, in the patent art, such` designation will -be employed fherein.

Similarly; while the magnesiumjoxide cementshaveV beenknown and used for many years, technical data conce'rning their .A precise composition has been not only kmeager but vague vand coniiicting', and..- over the years 'certain misconceptions concerningthe nature and char- 'acter of these cements'have arisen and have been accepted land'followedbyk those Working in the gart. Paramount among theseis the-belief'that these'cementsfare of nonhydraulie character in that they will not set under water. "This concept hasbeen yfirmly Ientrenched in the industry and the workers in the art have uniformly avoided pro- ','cedures and Ypractices which would increase the moisture 2,944,291 Patented July l2, 1960,

ice

quently, magnesium cement panels have hithertobeen manufactured by dry heat processes-in whichthe setting or curing of the cement occurs in a controlled atmosphere which prevents the absorption of moisture by the cement as therexothermic reaction takes place. In accordance with the @teachings of the aforementioned Collins patent, for example, it was'taughtthat the setting time of the magnesium cement could be reduced tofpractical limits for continuous `processing by preheating the Vbinder impregna'ted mat prior to compression in an atmosphere so controlled that it neither wet nor dried the mat to any substantial extent. While this procedure has been commercially practiced with good results, and has materially reduced the time `required to cause the cement to set, it nevertheless requires careful selection of the active oxide and the setting ltime is still such that it requires a press section having a length in excess of 100 feet even at relatively slow operating speeds.

The present invention is based upon our discovery that the magnesium oxide cements can be caused to set under conditions of extreme moisture content and that such cements are, infact, hydraulic in character. Coupled with this, we Ahave discovered that the ksetting time for such cementscan be accelerated by the saturation of the liberbinder mixture with live steam -to the point where the exothermic reaction takesplace and the binder sets within a matter of as little as 430 seconds. While we do not wish to. be limited by theory, itis our belief lthat the actual setting .ofthe magnesium oxide'takesplace substantially instantaneously atV the time the temperature of the binder reaches $212.?. F, Consequently, in accordance with our inventionLwe endeavor to heat the binder as rapidly as possiblesso as to cause the exothermic reaction of the binder to .take place as rapidly as possible. Once the `binder reaction has begun, it will carry through to completion on its: own accord, but by rapidly bringing the temperature ofthe binder to 2112/21?, Vthe natural reaction -isaccelerated and is, ,in fact, `drivenrto completion at the time the temperature of the material reaches V212i" F. 'fsteamhasunot'hitherto been employedl'as a setting medium for magnesium cement. `This has been `due in part 'tothe Aaccepted theory that the addition of moisture to the cement' was deleterious to the chemical reaction which takes place and in part to the fear .that the passage oflive'stearn through a-fiber-binder composition would cause undesirable erosion of--the binder.V YOur studies have showmhowever, that-steamecan be successfully used to accelerate--the-exothermic reaction of .the magnesium oxide provided certain critical ranges of operating conditions areobserved. For example, we have found that the, fvquality of the steam employed to saturate the mat isarkey` factor in ,the successful practice of our process i- 'and,;a`s ywillbe explained morer fully hereinafter, low

q'uality steam must'be employed: Our tests show that super-heated steam willnot Work satisfactorily.v Similarly, wehave fo'imdthat they line pressure of. the steam as'it passes/through the mat andthe duration of the steaming cycle are factors which have'a direct bearing .on ythe -physicalproperties 'of the nished product Yand hence must be properlyV controlled. f'- kln the light of the foregoing, it isa principal fobject of our invention'rto provide aprocess for the`rapid continuous 'manufacture of panels having a cementitious binder.` 1 Vs `A`further object of our invention is the provision 'of -a processjwherein live steam is utilized to accelerateand Vcarry togcompletion the exotherrnic reaction of a cement bonded librous structures whichrare particularlyadapted .for Vcontinuous productionwherein the material being formed can be compacted 'to 'size and caused to set in approximately 1 minute or less.

The foregoing, together with other objects of our invention which will appear hereinafter or will be apparent tothe skilled worker in the art upon reading these specilications, we accomplish'by those procedures and practices of which we shall now describe certain exemplary-embodiments.

'Reference is now made to the accompanying drawings wherein:

Figure lis a diagrammatic elevational view with parts broken away illustrating exemplary apparatus for steam treating Athe rbinder coated fibers in accordance with our invention.

In the practice of our process, we prefer to use a long ber Aspen eXcelsior as the brous material, although Aother Vliber may'be used inclusive of bagasse, straw, synthetics and the like. The binder is preferably composed of magnesium oxide and a gauging solution of water and magnesium sulphate. The fiber-binder composition will preferably have a binder to liber ratio of 55 parts binder to 45 parts liber, the parts being by Weight, although this ratio may Vary from 70-30 to 30-70 depending upon the 'fibers used; and the magnesium oxide to magnesium sulphate ratio will preferably be 65 parts oxide to 35 parts sulphate, although we have found that this ratio can vary from 40-60 to 80-20, the parts being by weight. Preferably the gauging liquid will consist of a 26% magnesium sulphate solution.

In the preparation of the binder, the gauging solution is prepared by adding the MgSO4.7H2O crystals to water. The magnesium oxide is then added to the gauging'solution and thoroughly mixed. After mixing, the binder is sprayed over the fibers which are then agitated, as by means of picker rolls, to thoroughly coat each fiber withV binder. The binder-coated fibers are then ready to be introduced into Va steam press and compacted to the desired thickness.

Insofar as the density of the board is concerned, it may be varied as desired throughout a range of about lbs. per cubic ft. to 50 lbs. per cubic ft., although we have found densities vin the range of lbs. per cubic ft. to 26 lbs. per cubic ft..produces board which is ideally suited for construction purposes. The amount of material required to make one board ft. of board (1.2" x 12" Vx 1") having a density of 21 lbs. per cubic ft. is as follows:

Where 15 lbs. per cubic foot -densty board is desired,

Vthe proportions will be `15/21 of those given above.

Where it is desired .to produce a board having a thickness of 2 or 3 inches, vthe Vmaterial amounts will be doubled or tripled, as the case may be, but the proportions will otherwise remain -the same. Similarly, if it is desired -to produce a board khaving a 26 lbs. percubic foot density, the amounts of material are increased by a ratio of 26/21 for the same volume of board.

Essentially, the press will comprise upper land lower perforated platen between which the liber-binder mixture is compacted to predetermined thickness, such as 1 inch, 2 inches or the like. The compressing pressure will be adjustable and will vary in accordance with ber density, cut and type of ber employed. For board having' a 15 Alb. per cubic foot density,the press pressure will be approximately 1200 lbs. 'per square foot, although the pressure range may vary from 8 00 lbs. per square foot to the aforementioned 1200 lbs. `Where 21 lb. density vis desired, ywe have Vfound a press pressure of 2000 lbs. iper square VVfoot t'o be highly'satisfactory.

Upon the compacting of the material to the desired thickness, `fit-iis then subjectedlto live Lsteam to effect Vthe 4 setting of the binder, the steam being introduced into the press through the perforations in the lower platen, forced through the mat, and evacuated through the upper platen. Preferably, the press will be heated prior to use so that its parts will be at substantially 212 F., thereby avoiding heat loss as the steam passes through the press. The heating of the press may be conveniently accomplished by enclosing it in a jacket or other insulated enclosure through whichhot air may becirculated, thereby preventing the metallic structure vfromsapping the heat generated by the steam and also preventing excessive condensation which would result were vthelive steamto be .introduced into a relatively cold press. A

The steam curing time may run anywhere rfrom 30 seconds to approximately `5 minutes. Of'course,'the actual steaming operation can be conducted for as long a time as desired, but beyond the necessary length of time to bring the internal temperature of the product to 212 F., the additional steaming time appears to be unnecessary. However, rsubsequent to the actual -time necessary to bring the internal temperature of ythe board to 212 VLF., we prefer to add a "soakingf AVcycle which is -in eect a safety factor. Thus 30 to -60 seconds may be added y:to the actual setting time (the time'required for the jgiroduct to reach 212 F.), -thereby assuring a vcomplete and full cure. Thus, curing time can be defined as the time :it takes the composition to g'o from 70 F. I(normal vvroom temperature) to 212 F. plus any additional Atir'newhich may be allowed for soaking, lthefsafety factor. "I'h'eno'rmal curing cycle will be from 1 minute to 1% minutes inclusive of the steaming Aand soaking periods.` One of the keys to the successful practice of our process is the use of low quality steam. Steam quality is a 'function of the moisture content of the steam. Generally speaking, any steam which Vis under quality, `i.e., contains more than 10% moisture, is considered low quality steam. Consequently, in accordance with our 'invention, we prefer to use steam which has a moisture content of 10% or more. Y

By way vof theory as to what happens `as the steam passes through the compacted material, the'steam carries a su'icient amount of moisture to surround the cement particles, condense upon them with a subsequent release of heat.A This released heat stimulates the exother'mic reaction of the 'magnesium oxide which in tu'rn generates additional heat which 'converts the condensate back "info stearn which is exhausted through the Upper'platen. The

use of low quality steam yconforms to our theory that an excess of moisture ,should be present to complete "the 'binder reaction. This'was 'confirmed'bytest inwwliich 'super-heated 'steam (steam which has 'substantially n`o moisture content) Wasused in place of low quality'stem. It was found that with super-heated steam,"poor esults were achieved and in many instances the binder was found vto remain unbonded. Similar unsatisfactory re sults were noted kin products formed with Vsteam 'off a kquality above 90% although the diferencesnoted'vaiietl with the length of the steaming cycle.

There is no practical lower limit vto the quality of'thfe steam which may be successfully used. The' process' 'may be carried to the ultimate using 0% stearn4boi1ing'wate'r. ln other words, rather than using live steam as the curing medium, hot water may be used, the water `beinfgb`rol`1ght just toits boiling point butshort of the stageof altu'rbulent boiling condition. Test samples in whichthe material Vwas submerged in boiling `or `near boiling water were found to set vas effectively as where the material wassubjected to live steam; and theproperties of the water `set product were substantially the-same as thoseofthe steam set product.

The steam kpressure at the time the 'steam vis introduced into the press may vary from 5 lbs. per square inch to 90 lbs. .per square inch without producing excessive binder erosion. We prefer to l'operatewithinthe range of `10 Yto 1.15 lbs. pervsquare inchgauge pressure. Within :this range optimum results are obtained insofaras the physical properties of the product are concerned. Y .Y y

Referring now tothe drawings, Ywe have therein illustrated an' exemplary device by means of which our process may be practiced'to produce board inl a continuous operation. As seen' in the drawing, the bers 1' are-'delivered from a hopper or chutevZ onto a moving conveyor vb elt 3 where the fibers are formed into a mat and sprayed with binder from a spray-head 4 arranged transversely with respect to the conveyor belt 3. It will vbe understood that the apparatus illustrated for depositing the fibers on the conveyor is diagrammatic only and'we :prefer to process the fibers in accordance with theteachings of Collins United States Patent No. 2,744,045, Apparatus and Process forV Continuously Feeding and Spraying Wood Wool and Like Materials, which teaches apparatus and procedures for beating and coating the fibers, including such steps as ufling the initially compacted and baled iibers, establishing a uniform ow of the tiuied material and depositing it in a uniform manner on a conveying means, coating the fibers with the binder material and depositing the coatedA fibers on the continuously moving conveyor 3 in the form of a mat which is conducted/to thepress. v

YThe conveyor delivers the mat to the press 5 where the mat is compacted-to form the matted material into a layer of predetermined thickness. The press is composed of upper and lower conveyor belts 6 and 7, respectively, the belts being of foraminous character, preferably formed of stainless steel perforated on 1/2" centers, andbacked up by a series of cast iron flights 8 and 9 which extend crosswise with respect to the length'of the press and linked together for continuous movement in synchronism with the movement of the belts 6 and 7. It will be understood that the flights 8 and 9 will be adjustably mounted so that the distance between the upper and lower nights may be Varied in accordance with the desired thickness of the compressed product.

A manifold 10 underlies the lower iiight 9, the manifold 10 having elongated openings in its upper surface whichcommunicate with openings in the under surfaces of the flights 9. Live steam is fed through pipe 11 into the manifold, the steam passing upwardly from the manifold into the flights 9. The upper surfaces of the flights are Ain the form of a grating or grill through which the steam will pass upwardly throughy the perforations in belt 7 and into the compacted material. The upper flights 8 are similar to the lower flight excepting they communicate with an exhaust manifold 12, the arrangement being such that the steam passing through the mat will be evacuated through the upper ghts 8 into the exhaust manifold 12. Preferably, the exhaust manifold will be of a length several times that of the steam manifold 10 so that the evacuation of steam and moisture from the mat may continue subsequent to the termination of the actual steam application. The steam will be exhausted from the manifold through exhaust stack 13 having a blower 14.

As the mat moves through the press, the magnesium cement will be set sufficiently to maintain the thickness formed by the press, so that when the mat leaves the press it will not swell or expand, but will remain at the dimension established by the press. Upon passage of the formed mat from the press, the mat will be passed through one or more drying ovens wherein heated air is circulated to remove additional moisture from vthe mat land cause it to thoroughly dry. The mat may be cut into 6 Besides speeding up production, stearn curing also has benecial elects onthe finished product, as evidenced by the following comparison of steamcured samples to samplescured by presentdry cure methods.

l Cdmparisorifof d ry cure with steam cure 1 l Averages of 10 control samples.r

i 45 sec. steam period, 15 sec. soaking, 52% quality steamat a pressure of 10 p.s.i.g. (lbs. per square inch gauge). n

,t Hot air at 180 F.

Microscopic examination of steam cured and cured board shows no material differences between the two forms and the coverage of the fibers is substantially the same. All tests indicate that board formed in accord- `ance with our invention has physical and chemical properties which are either superior or equal to board formed by presently known dry cure methods. Our process has materially reduced production time which has in turn enabled us to materially reduce the size and cost of the equipment'required for processing the board. At the same time, the relative chemical activity of the magnesium oxide has been rendered unimportant, thereby permitting the use of a wider range of oxides which are more readily available and less expensive.

Having thusk described our invention in certain exemplary embodiments, what we desire to secure and protect by Letters Patent is:

1. The method of forming a low density porous panel composed of fibrous material and a magnesium cement binder composed of water-borne magnesium oxide and magnesium salts of the group of sulphate and chloride, said binderbeing settable upon hydration by an exothermic reaction, which method consists essentially of forming a porous layer of fibers each of which is thoroughly coated with said cementitious binder, compacting the porous layerI so formed between compressing surfaces and, while holding the layer between said compressing surfaces, saturating said porous layer with an aqueous fluid at a temperature of substantially 212 F. so as to rapidly bring said layer to an internal temperature 0f substantially 212 F. under conditions Aof excessive moisture, whereby to rapidly accelerate and carry to completion the exothermic reaction of said cement binder to set said layer against expansion while holding it between said compressing surfaces.

2. The method claimed in claim 1 wherein the berbinder ratio is substantially 45% ber to 55% binder on a weight basis.

3. The method claimed in claim 1 wherein the ratio of magnesium oxide'to magnesium salts is from 40-60 to -20 parts by weight.

v4. The method claimed in claim 1 wherein the compacted layer is rapidly heated by means of steam injected in said layer while held between said compressing surfaces.

5. The method claimed in claim 4 wherein said steam is of low quality, having a moisture content of at least 10%.

6. The method claimed in claim 5 wherein said layer is subjected to low quality steam for at least 30 seconds and not more than substantially 5 minutes.

7. The method claimed in claim 6 wherein, subsequent to the passage of said low quality steam through said layer, said layer is retained between said compressing surfaces for a soaking period, followed by its removal from between saidcompressing surfaces.

8. The method claimed in claim 7 wherein said layer has a density of substantially 15 lbs. per cubic foot, and

7 wherein said layer is compacted under a pressure of from 800 to 1200 lbs. per'squarerfoot.

9. A method forvproducing a panel composed ofmagnesium cement and lwood bres, which comprises forming a layer of bers impregnated with Water-borne magnesium'oXide and magnesium salts of the group of the sulphate and chloride, compressing the layer so formed between compressing surfaces at least one of which is of a foraminous character and, while the layer is so compressed, subjecting it to live steam having a moisture content of at least 10% and a line pressure of notmore than 90'1bs. per square inch gauge.

10. The method claimed-in claim 9 wherein said layer is subjected -tosaid live steam for la period of fromabout 30 seconds to about 5 minutes.

1l. A method for rapidly and continuously forming cement bonded brous panels wherein a layer of bers impregnated with a mixture of water-borne magnesium oxide and magnesium 'salts or the ygroup of sulphate and chloride is continuously moved between compressing Ysurfaces, theistep `which comprises causingsaid layer to set while held between said compressing surfaces by subjecting these :layers to wet live steam for at least 30 seconds ata line pressure of at least lbs. per square'inch gauge and not more than 90 lbs. per square inch gauge.

l2. A method of rapidly forming a cement bonded brous ,panelwherein a layer ofibers thoroughly coated with 'a mixture consisting essentiallyof water-'borne magnesium -oxide .and magnesium salt of thergroup ofrsulphate and vchloride fis compacted under `pressure to predetermined .thicknes's, the step which consists in passing wetlive steam :through the compacted'layerjfora period of timesucientto bring the internal temperature of said layer to 21.2 F., whereby to force Ythe exothermic reaction-oisaid .magnesium oxide-magnesium salt mixture to completionand cause said layer-to set in its compacted condition.

13. The .method .claimed in claim 12 `.wherein said steamis of not more than quality .and is introduced into saidilayerat aline pressure .of not more than 90 lbs. persquare inch gauge.

:References {Cited in :the :leo'f .this Ypatent 'UNITED STATES PATENTS .1,990,554 .Libberton Feb. 12, (1935 2,3 10,128 Smith Feb. 2, 1943 `2,543,752 ,Austin et al. .Mar. 6, 1951 2,635,301 Schubertet a1. Apr. ,21, .1953 2,655,458 Collins i Oct. 13, 1953 V.2,698,260 Meauzeetlal Dec. 28, 1954 .2,703,762 Slayter .Man 8, 1955 

1. THE METHOD OF FORMING A LOW DENSITY POROUS PANEL COMPOSED OF FIBROUS MATERIAL AND A MAGNESIUM CEMENT BINDER COMPOSED OF WATER-BORNE MAGNESIUM OXIDE AND MAGNESIUM SALTS OF THE GROUP OF SULPHATE AND CHLORIDE, SAID BINDER BEING SETTABLE UPON HYDRATION BY AN EXOTHERMIC REACTION, WHICH METHOD CONSISTS ESSENTIALLY OF FORMING A POROUS LAYER OF FIBRES EACH OF WHICH IS THOROUGHLY COATED WITH SAID CEMENTITIOUS BINDER, COMPACTING THE POROUS LAYER SO FORMED BETWEEN COMPRESSING SURFACES AND, WHILE HOLDING THE LAYER BETWEEN SAID COMPRESSING SURFACES, SATURATING SAID POROUS LAYER WITH AN AQUEOUS FLUID AT A TEMPERATURE OF SUBSTANTIALLY 212% F. SO AS TO 